CN103441194A - LED epitaxial wafer, manufacturing method thereof and LED chip with same - Google Patents
LED epitaxial wafer, manufacturing method thereof and LED chip with same Download PDFInfo
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Abstract
The invention discloses an LED epitaxial wafer, a manufacturing method of the LED epitaxial wafer and an LED chip with the LED epitaxial wafer. The manufacturing method of the LED epitaxial wafer includes the following steps of sequentially and outward forming a U type GaN layer, an N type GaN layer, a quantum well layer, a first P type GaN layer, a second P type GaN layer and a third P type GaN layer from the surface of a substrate, and further includes the annealing steps, wherein the annealing steps include at least one annealing step conducted after the first P type GaN layer is formed and before the third P type GaN layer is formed, and another annealing step conducted after the third P type GaN layer is formed. According to the manufacturing method of the LED epitaxial wafer, the hole concentration of the LED chip can be improved, defects of the surfaces of the P type GaN layers and the defects of the inner portions of the P type GaN layers are eliminated, the luminance of the LED chip is improved, and the driving voltage is lowered.
Description
Technical field
The present invention relates to technical field of semiconductor illumination, in particular to a kind of LED epitaxial wafer, its manufacture method and comprise its LED chip.
Background technology
GaN sill (comprising GaN, AlGaN, InGaN, MgGaN, SiGaN) belongs to direct gap semiconductor, and its band gap is adjustable continuously from 1.8～6.2V, be the most frequently used material of producing brightness blue light, green glow and white light LEDs, be widely used in backlight, the demonstration of large scale screen, indicate the fields such as label indication, signal lamp and illumination.But gallium nitride based LED exists that luminous efficiency is low, the high deficiency of driving voltage.In order to realize more high efficiency, more high brightness, the gallium nitride based LED of low driving voltage more, need to reduce the series resistance in gallium nitride based LED, and the electrode dopant activation efficiency in series resistance and LED epitaxial wafer is closely related.
At present, the manufacture method of GaN base LED epitaxial wafer is generally: adopt MOCVD(metallo-organic compound chemical gaseous phase depositing process) epitaxial growth one deck GaN resilient coating on Sapphire Substrate; And then the GaN of the non-doping of growing, purpose is to improve the quality of follow-up epitaxial crystal, on this basis the GaN quantum well of the N-type GaN of grow doping Si, doping In successively again; Finally, growth P-type GaN hole injection layer, P type GaN electronic barrier layer and high temperature P type GaN layer, the P type GaN of formation doped with Mg or Al.
In the growth course of LED epitaxial wafer, in N-type GaN, alloy Si has up to 1E+21atom/cm
3activation concentration, thereby make N-type GaN there is lower resistivity; The dopant that P type GaN is commonly used is Mg, yet mix the N-type GaN obtained after Mg and have higher resistivity, be mainly due to Mg can be under the high growth temperature atmosphere ammonia decompose the H produced and be combined and form inactive Mg-H complex compound, the passivation by H loses activity Mg, make the activation efficiency of Mg very low, general carrier concentration only accounts for 0.1%～1% of doping content.In the LED device, the hole concentration in P type GaN layer is only 1.0E+17～1.2E+17atom/cm at present
3, than low 2～3 orders of magnitude of doping content.
In order to improve the hole concentration in P type GaN layer, existing technique is annealed usually after growth P-type GaN, thereby destroys the Mg-H key and activate alloy.But, thicker due to P layer GaN layer, its thickness is 240nm～310nm, and interrupting of Mg-H key needs the regular hour, make away from surperficial activation degree lower than near surperficial P layer activation degree, cause the activity ratio of Mg of hole injection layer and electronic barrier layer on the low side.Although improve the activation degree that annealing time can improve whole P type GaN layer, high temperature is annealed for a long time and can be destroyed the structure on P type GaN top layer.
Summary of the invention
The present invention aims to provide a kind of LED epitaxial wafer, its manufacture method and comprises its LED chip, to solve the too low technical problem of hole concentration of P type GaN layer in existing LED device.
One aspect of the present invention provides a kind of manufacture method of LED epitaxial wafer.This manufacture method comprises: at substrate surface, outwards form successively U-shaped GaN layer, N-type GaN layer, quantum well layer and a P type GaN layer, the 2nd P type GaN layer and the 3rd P type GaN layer; Annealing steps, this annealing steps comprises: after forming a P type GaN layer, form the annealing steps at least one times carried out before the 3rd P type GaN layer; Forming another annealing steps carried out after the 3rd P type GaN layer.
Further, in above-mentioned annealing steps: after forming a P type GaN layer, to form the annealing steps carried out before the 3rd P type GaN layer be one or many, when this annealing steps is one time, its duration is not less than 120s; When this annealing steps, for repeatedly the time, repeatedly total duration of annealing steps is no more than 360s, and the duration of single annealing steps is not less than 120s; In another annealing steps carried out after forming the 3rd P type GaN layer, the time of annealing is 15～25min.
Further, above-mentioned annealing steps comprises: carry out the first annealing steps after forming a P type GaN layer, preferably, the first annealing steps comprises: in temperature, be 750～760 ℃, and the N that pressure is 200～300mbar
2be incubated 240～300s under atmosphere; Carry out the second annealing steps after forming the 3rd P type GaN layer, preferably, the second annealing steps comprises: be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 20～25min under atmosphere.
Further, above-mentioned annealing steps comprises: carry out the first annealing steps after forming the 2nd P type GaN layer, preferably, the first annealing steps comprises: be cooled to 760～800 ℃ by 40～60s, the N that is 600～800mbar at pressure
2be incubated 300～360s under atmosphere; Carry out the second annealing steps after forming the 3rd P type GaN layer, preferably, the second annealing steps comprises: being cooled to 730～780 ℃ by 300～320s, is 600～800mbar N at pressure
2be incubated 20～25min under atmosphere.
Further, above-mentioned annealing steps comprises: carry out the first annealing steps after forming a P type GaN layer, preferably, the first annealing steps comprises: in temperature, be 750～760 ℃, and the N that pressure is 200～300mbar
2be incubated 120～150s under atmosphere; Carry out the second annealing steps after forming the 2nd P type GaN layer, preferably, the second annealing steps comprises: be cooled to 760～800 ℃ by 40～60s, the N that is 600～800mbar at pressure
2be incubated 150～180s under atmosphere; Carry out the 3rd annealing steps after forming the 3rd P type GaN layer, preferably, the 3rd annealing steps comprises: be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 15～20min under atmosphere.
Further, a P type GaN layer is the P type GaN layer of mixing Mg that thickness is 50～60 nanometers, and wherein the doping content of Mg is 7E+19～1E+20atom/cm
3; The 2nd P type GaN layer is the P type GaN layer of mixing Al and Mg that thickness is 40～50 nanometers, and wherein the doping content of Al is 1E+20～2E+20atom/cm
3, the doping content of Mg is 1E+19～2E+19atom/cm
3; The 3rd P type GaN layer is the P type GaN layer of mixing Mg that thickness is 150～200 nanometers, and wherein the doping content of Mg is 1E+19～5E+19atom/cm
3.
Further, the step that forms a P type GaN layer comprises by 40～50s and is cooled to 750～760 ℃, the N that is 200～300mbar at pressure
2under atmosphere, a P type GaN layer of magnesium is mixed in growth; The step that forms the 2nd P type GaN layer comprises by 70～90s and is warming up to 920～970 ℃, the N that is 150～300mbar at pressure
2under atmosphere, the 2nd P type GaN layer of Al and Mg is mixed in growth; The step that forms the 3rd P type GaN layer comprises by 60～70s and is warming up to 1000～1100 ℃, the N that is 200～600mbar at pressure
2under atmosphere, the 3rd P type GaN layer of Mg is mixed in growth.
Another aspect of the present invention is to provide a kind of LED epitaxial wafer, and this LED epitaxial wafer is made by the manufacture method of LED epitaxial wafer provided by the present invention.
Another aspect of the present invention is to provide a kind of LED chip, comprises epitaxial wafer, P electrode, N electrode and protective layer, and wherein, above-mentioned epitaxial wafer is LED epitaxial wafer provided by the present invention.
The present invention has following beneficial effect: the present invention by increasing annealing steps at least one times after forming a P type GaN layer, before forming the 3rd P type GaN layer, make the thermal vibration aggravation of the H atom in a P type GaN layer or a P type GaN layer and the 2nd P type GaN layer, the Mg-H key is interrupted fully, and Mg has obtained activation; In the annealing steps process of carrying out after forming the 3rd P type GaN layer, the thermal stress in whole P type GaN layer becomes very little, thereby makes the atomic heat vibration in P type GaN layer more even, and the Mg in P type GaN layer is effectively activated.Hole concentration in the LED chip obtained by method provided by the invention is improved, and P type GaN layer is surperficial and inner defect is eliminated, and crystalline quality is improved.
The accompanying drawing explanation
The accompanying drawing that forms a part of the present invention is used to provide a further understanding of the present invention, and schematic description and description of the present invention the present invention does not form inappropriate limitation of the present invention for explaining.In the accompanying drawings:
Fig. 1 shows the test result comparison diagram of the LED product brightness that the embodiment of the present invention 1 and Comparative Examples 1 provide;
Fig. 2 shows the test result comparison diagram of the LED product driving voltage that the embodiment of the present invention 1 and Comparative Examples 1 provide; And
Fig. 3 shows the test result comparison diagram of the LED product hole concentration that the embodiment of the present invention 1 and Comparative Examples 1 provide.
Embodiment
Below, describe in more detail according to exemplary embodiment of the present invention with reference to the accompanying drawings.Yet these exemplary embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to the embodiments set forth herein.To should be understood that, to provide these embodiment of the present inventionly to disclose thoroughly and complete in order making, and the design of these exemplary embodiments is fully conveyed to those of ordinary skills.But the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
From background technology, there is the too low technical problem of hole concentration of P type GaN layer in existing LED device, the present inventor is studied the problems referred to above, and a kind of manufacture method of LED epitaxial wafer is provided.This manufacture method is included in the step that substrate surface outwards forms U-shaped GaN layer, N-type GaN layer, quantum well layer and a P type GaN layer (being hole injection layer), the 2nd P type GaN layer (being electronic barrier layer) and the 3rd P type GaN layer (being high temperature P type GaN layer) successively, also comprise annealing steps, this annealing steps comprises simultaneously: after forming a P type GaN layer, form the annealing steps at least one times carried out before the 3rd P type GaN layer; Forming another annealing steps carried out after the 3rd P type GaN layer.
Preferably, in the annealing steps of the manufacture method of above-mentioned LED epitaxial wafer, after forming a P type GaN layer, to form the annealing steps carried out before the 3rd P type GaN layer be one or many, when this annealing steps is one time, its duration is not less than 120s; When this annealing steps, for repeatedly the time, repeatedly total duration of annealing steps is no more than 360s, and the duration of single annealing steps is not less than 120s; In another annealing steps carried out after forming the 3rd P type GaN layer, the time of annealing is 15～25min.
In the growth course of the P type GaN layer that has the LED epitaxial wafer now, the H that doped with Mg can produce with ammonia (one of GaN reaction raw materials) decomposition is combined and is formed inactive Mg-H complex compound, make Mg lose activity, the activation efficiency step-down of Mg, the hole concentration in P type GaN layer is step-down also.In the manufacturing process of LED epitaxial wafer of the present invention, by after forming a P type GaN layer, before forming the 3rd P type GaN layer, carrying out annealing steps at least one times, make the thermal vibration aggravation of the H atom in a P type GaN layer or a P type GaN layer and the 2nd P type GaN layer, the Mg-H key is interrupted fully, Mg has obtained activation, thereby has improved concentration and the uniformity in hole; Simultaneously, the atom on a P type GaN layer or a P type GaN layer and the 2nd P type GaN layer surface is reset, and surperficial and inner defect is eliminated, and crystalline quality is improved.
After above-mentioned annealing in process, the thermal stress of a P type GaN layer or a P type GaN layer and the 2nd P type GaN layer inside is eliminated to a great extent, and most of Mg has obtained activation.Therefore, in the annealing steps process of carrying out after forming the 3rd P type GaN layer, thermal stress in whole P type GaN layer becomes very little, thereby make the atomic heat vibration in P type GaN layer more even, Mg in P type GaN layer is effectively activated, and then the brightness that has improved the LED epitaxial wafer, reduced the driving voltage of LED epitaxial wafer.
In the manufacture method of the above-mentioned LED epitaxial wafer of the present invention, annealing steps can adopt existing annealing way, in a kind of preferred implementation of the present invention, this annealing steps comprises: after forming a P type GaN layer, carry out the first annealing steps, wherein the first annealing steps is to be 750～760 ℃ in temperature, the N that pressure is 200～300mbar
2be incubated 240～300s under atmosphere; Carry out the second annealing steps after forming the 3rd P type GaN layer, wherein the second annealing steps is for to be cooled to 730～780 ℃ by 300～320s, the N that pressure is 600～800mbar
2be incubated 20～25min under atmosphere.
In above-mentioned preferred implementation, the first annealing steps carries out after completing a P type GaN layer growth, it can make the thermal vibration aggravation of the H atom in a P type GaN layer, the Mg-H key is interrupted fully, and then improved the activity ratio of Mg in a P type GaN layer (being hole injection layer), and reduced the lattice defect in the hole injection layer, made the mobility of the sub-trap of hole vectors in hole injection layer be increased; The second annealing steps has further improved the activity ratio of Mg in whole P type GaN layer.Under the acting in conjunction of twice annealing step, the brightness of LED epitaxial wafer is improved, and driving voltage is reduced.
In another preferred implementation of the present invention, annealing steps comprises: carry out the first annealing in process after forming the 2nd P type GaN layer, the step of the first annealing in process is for to be cooled to 760～800 ℃ by 40s～60s, the N that is 600～800mbar at pressure
2be incubated 300～360s under atmosphere; Carry out the second annealing in process after forming the 3rd P type GaN layer, wherein the step of the second annealing in process is for to be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 20～25min under atmosphere.
In above-mentioned preferred implementation, the first annealing steps is to complete first, after the 2nd P type GaN layer growth, carry out, and the time of this first annealing steps is a bit larger tham the time of the first annealing steps in above-mentioned preferred implementation, this first annealing steps has improved the activity ratio of Mg in a P type GaN layer (being hole injection layer) and the 2nd P type GaN layer (being electronic barrier layer), can make the mobility of the sub-trap of hole vectors in hole injection layer be increased, can prevent again hole in electronic barrier layer due to N-type GaN layer in electron recombination be consumed totally, the second annealing steps has further improved the activity ratio of Mg in whole P type GaN layer.Under the acting in conjunction of twice annealing step, the brightness of LED epitaxial wafer is improved, and driving voltage is reduced.
In another preferred implementation of the present invention, above-mentioned annealing steps comprises: carry out the first annealing in process after forming a P type GaN layer, wherein the step of the first annealing in process is to be 50～760 ℃ in temperature, the N that is 200～300mbar at pressure
2be incubated 120～150s under atmosphere; Carry out the second annealing in process after forming the 2nd P type GaN layer, wherein the step of the second annealing in process is for to be cooled to 760～800 ℃ by 40s～60s, the N that is 600～800mbar at pressure
2be incubated 150～180s under atmosphere; Carry out the 3rd annealing in process after forming the 3rd P type GaN layer, wherein the step of the 3rd annealing in process is: be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 15～20min under atmosphere.
In above-mentioned preferred implementation, carried out annealing steps three times in P type GaN layer growth process, carry out the first annealing steps after completing a P type GaN layer growth, carry out the second annealing steps after completing the 2nd P type GaN layer growth, after having completed the 3rd P type GaN layer growth, carry out the 3rd annealing steps; Although above-mentioned three annealing steps can make technique become complicated, and may there is the uncertain factor that affects P type GaN layer growth quality, but under the effect of above-mentioned three annealing steps, in whole P type GaN layer, the Mg-H key is interrupted fully, the activity ratio of Mg is improved more fully, thereby make the brightness of LED epitaxial wafer be improved, driving voltage is reduced.
In the manufacture method of LED epitaxial wafer provided by the present invention, the growth of first, second, third P type GaN layer can adopt the growth pattern of existing P type GaN layer, in a kind of preferred implementation of the present invention, the growth step of this first, second, third P type GaN layer comprises:
Be cooled to 750～760 ℃ by 40～50s, the N that is 200～300mbar at pressure
2under atmosphere, a P type GaN layer of magnesium is mixed in growth, and wherein the thickness of a P type GaN layer is 50～60 nanometers, and the doping content of Mg is 7E+19～1E+20atom/cm
3.;
Be warming up to 920～970 ℃ by 70～90s, the N that is 150～300mbar at pressure
2under atmosphere, the 2nd P type GaN layer of Al and Mg is mixed in growth, and the doping content that wherein thickness of the 2nd P type GaN layer is 40～50, Al is 1E+20～2E+20atom/cm
3, the doping content of Mg is 1E+19～2E+19atom/cm
3;
Be warming up to 1000～1100 ℃ by 60～70s, the N that is 200～600mbar at pressure
2under atmosphere, the 3rd P type GaN layer of Mg is mixed in growth, and wherein the thickness of the 3rd P type GaN layer is 150～200 nanometers, and the doping content of Mg is 1E+19～5E+19atom/cm
3.
Above-mentioned growth technique can include but not limited to chemical vapour deposition (CVD), sputter, heat deposition, and above-mentioned preparation technology is the common technological means in this area, does not repeat them here.
In a kind of optimal way of the manufacture method of LED epitaxial wafer provided by the present invention, the step that forms successively U-shaped GaN layer, N-type GaN layer, quantum well layer on substrate comprises:
Be warming up to 1000～1150 ℃ by 480～500 seconds from room temperature, process Sapphire Substrate 5～6min under the condition that is 150～200mbar at hydrogen atmosphere, pressure;
Be cooled to 540～590 ℃ by 400～450 seconds, pressure is controlled at 450～600mbar, the GaN resilient coating that is 30～45nm at Grown on Sapphire Substrates thickness;
Be warming up to 1050～1150 ℃ by 320～380 seconds, pressure is controlled at 450～600mbar, continues the GaN that undopes of growth 2.5～3.5um, and above-mentioned GaN resilient coating and the GaN that undopes form U-shaped GaN layer;
Keep temperature-resistant, pressure is controlled at 200～400mbar, the N-type GaN layer of 3.0～3.5 μ m doped silicons of then growing, wherein the doping content 5E+18 of silicon～1E+19atom/cm in the first N-type GaN
3;
Be cooled to 740～840 ℃ by 240～300 seconds, pressure is controlled at 300～400mbar, the InxGa(1-x that periodically growth thickness is 2.7～3.5nm) the GaN barrier layer that N(x=0.20～0.22) potential well layer and thickness are 11～12nm, form quantum well layer, the gross thickness of described quantum well layer is 165～233nm.
Simultaneously, the present invention also provides a kind of LED epitaxial wafer obtained according to the manufacture method of above-mentioned LED epitaxial wafer.In this epitaxial wafer, P type GaN layer has higher hole concentration, makes the brightness of this LED epitaxial wafer be improved, and driving voltage is reduced.
In addition, the present invention also provides a kind of LED chip obtained according to the manufacture method of above-mentioned LED chip.In this LED chip, P type GaN layer has higher hole concentration, makes the brightness of this chip be improved, and driving voltage is reduced.
Below will further illustrate LED epitaxial wafer provided by the present invention, LED chip and their manufacture method with specific embodiment.
Embodiment 1
The present embodiment provides a kind of manufacture method of LED chip, and this manufacture method comprises the following steps:
Step S1 forms successively GaN resilient coating, U-shaped GaN layer, N-type GaN layer, quantum well layer on substrate, comprises the following steps:
Be warming up to 1100 ℃ by 500 seconds from room temperature, under the condition that is 170mbar at hydrogen atmosphere, chamber pressure, process Sapphire Substrate 6 minutes;
Be cooled to 550 ℃ by 440 seconds, chamber pressure is controlled at 500mbar, the GaN resilient coating that is 40nm at Grown on Sapphire Substrates thickness;
Be warming up to 1100 ℃ by 350 seconds, chamber pressure is controlled at 500mbar, continues the GaN that undopes of growth 2.5 μ m, i.e. U-shaped GaN layer;
Keep temperature-resistant, chamber pressure is controlled at 350mbar, the N-type GaN layer that then growth thickness is 3.5 μ m doped silicons, wherein the doping content 7.6E+18atom/cm of silicon
3;
Be cooled to 800 ℃ by 250 seconds, chamber pressure is controlled at 400mbar, the InxGa(1-x that alternating growth thickness is 3nm) N(x=0.22) GaN barrier layer that potential well layer and thickness are 12nm, growth cycle is 15, forms quantum well layer.
Step S2 forms successively a P type GaN layer, the 2nd P type GaN layer and the 3rd P type GaN layer, and is annealed on quantum well layer, specifically comprises the following steps:
Be cooled to 750 ℃ by 40s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 50 nanometers, wherein the doping content of Mg is 7E+19atom/cm
3;
Carry out the first annealing, concrete technology is: keep temperature and pressure constant, at N
2be incubated 240s under atmosphere;
Be warming up to 920 ℃ by 70s, chamber pressure is controlled at 150mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 40 nanometers, wherein the doping content of Al is 1E+20atom/cm
3, the doping content of Mg is 1E+19atom/cm
3;
Be warming up to 1000 ℃ by 60s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 150 nanometers, wherein the doping content of Mg is 1E+19atom/cm
3;
Carry out the second annealing, concrete technology is: be cooled to 730 ℃ by 300s, chamber pressure is that 600mbar is at N
2be incubated 20min under atmosphere.
Step S3 makes P electrode, N electrode and protective layer on the LED epitaxial wafer, comprises the following steps:
Make P, N electrode pattern by photoetching and etching technics, then evaporation Cr/Pt/Au electrode layer, form P electrode and N electrode, finally on exposure machine, makes P, N electrode parcel pattern, and the protective layer that evaporation thickness is 50nm, obtain LED chip.
Embodiment 2
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 760 ℃ by 50s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 60 nanometers, wherein the doping content of Mg is 1E+20atom/cm
3;
Carry out the first annealing, concrete technology is: keep temperature and pressure constant, at N
2be incubated 300s under atmosphere;
Be warming up to 970 ℃ by 90s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 50 nanometers, wherein the doping content of Al is 2E+20atom/cm
3, the doping content of Mg is 2E+19atom/cm
3;
Be warming up to 1100 ℃ by 70s, chamber pressure is controlled at 600mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 200 nanometers, wherein the doping content of Mg is 5E+18atom/cm
3;
Carry out the second annealing, concrete technology is: be cooled to 780 ℃ by 320s, chamber pressure is that 800mbar is at N
2be incubated 25min under atmosphere.
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 750 ℃ by 40s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 50 nanometers, wherein the doping content of Mg is 7E+19atom/cm
3;
Be warming up to 920 ℃ by 70s, chamber pressure is controlled at 150mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 40 nanometers, wherein the doping content of Al is 1E+20atom/cm
3, the doping content of Mg is 1E+19atom/cm
3;
Carry out the first annealing, concrete steps are: be cooled to 760 ℃ by 40s, chamber pressure is controlled at 600mbar, at N
2be incubated 300s under atmosphere;
Be warming up to 1000 ℃ by 60s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 150 nanometers, wherein the doping content of Mg is 1E+19atom/cm
3;
Carry out the second annealing, concrete steps are: be cooled to 730 ℃ by 300s, chamber pressure is 600mbar, at N
2be incubated 20min under atmosphere.
Embodiment 4
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 760 ℃ by 50s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 60 nanometers, wherein the doping content of Mg is 1E+20atom/cm
3;
Be warming up to 970 ℃ by 90s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 50 nanometers, wherein the doping content of Al is 2E+20atom/cm
3, the doping content of Mg is 2E+19atom/cm
3;
Carry out the first annealing, concrete steps are: be cooled to 800 ℃ by 60s, chamber pressure is controlled at 800mbar, at N
2be incubated 360s under atmosphere;
Be warming up to 1100 ℃ by 70s, chamber pressure is controlled at 600mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 200 nanometers, wherein the doping content of Mg is 5E+18atom/cm
3;
Carry out the second annealing, concrete steps are: be cooled to 780 ℃ by 320s, chamber pressure is 800mbar, at N
2be incubated 25min under atmosphere.
Embodiment 5
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 750 ℃ by 40s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 50 nanometers, wherein the doping content of Mg is 7E+19atom/cm
3;
Carry out the first annealing in process, concrete steps are: keep temperature, pressure constant, N
2be incubated 120s under atmosphere;
Be warming up to 920 ℃ by 70s, chamber pressure is controlled at 150mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 40 nanometers, wherein the doping content of Al is 1E+20atom/cm
3, the doping content of Mg is 1E+19atom/cm
3;
Carry out the second annealing, concrete steps are: be cooled to 760 ℃ by 40s, chamber pressure is controlled at 600mbar, at N
2be incubated 150s under atmosphere;
Be warming up to 1000 ℃ by 60s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 150 nanometers, wherein the doping content of Mg is 1E+19atom/cm
3;
Carry out the 3rd annealing, concrete steps are: be cooled to 730 ℃ by 300s, chamber pressure is 600mbar, at N
2be incubated 15min under atmosphere.
Embodiment 6
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 760 ℃ by 50s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 60 nanometers, wherein the doping content of Mg is 1E+20atom/cm
3;
Carry out the first annealing in process, concrete steps are: keep temperature, pressure constant, under the N2 atmosphere, be incubated 150s;
Be warming up to 970 ℃ by 90s, chamber pressure is controlled at 300mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 50 nanometers, wherein the doping content of Al is 2E+20atom/cm
3, the doping content of Mg is 2E+19atom/cm
3;
Carry out the second annealing, concrete steps are: be cooled to 800 ℃ by 60s, chamber pressure is controlled at 800mbar, at N
2be incubated 180s under atmosphere;
Be warming up to 1100 ℃ by 70s, chamber pressure is controlled at 600mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 200 nanometers, wherein the doping content of Mg is 5E+18atom/cm
3;
Carry out the 3rd annealing, concrete steps are: be cooled to 780 ℃ by 320s, chamber pressure is 800mbar, at N
2be incubated 20min under atmosphere.
Embodiment 7
The present embodiment provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
Step S2 is in the present embodiment:
Be cooled to 765 ℃ by 55s, chamber pressure is controlled at 190mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 48 nanometers, wherein the doping content of Mg is 6.8E+19atom/cm
3;
Carry out the first annealing in process, concrete steps are: keep temperature, pressure constant, N
2be incubated 170s under atmosphere;
Be warming up to 980 ℃ by 95s, chamber pressure is controlled at 320mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 55 nanometers, wherein the doping content of Al is 2.2E+20atom/cm
3, the doping content of Mg is 2.2E+19atom/cm
3;
Carry out the second annealing, concrete steps are: be cooled to 750 ℃ by 70s, chamber pressure is controlled at 820mbar, at N
2be incubated 200s under atmosphere;
Be warming up to 1110 ℃ by 50s, chamber pressure is controlled at 620mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 145 nanometers, wherein the doping content of Mg is 5.2E+19atom/cm
3;
Carry out the 3rd annealing, concrete steps are: be cooled to 790 ℃ by 330s, chamber pressure is 820mbar, at N
2be incubated 25min under atmosphere.
Comparative Examples 1
This Comparative Examples provides a kind of manufacture method of LED epitaxial wafer, and wherein step S1 is identical with embodiment 1 step S1, and step S3 is identical with the step S3 in embodiment 1.
In this Comparative Examples, step S2 is:
Form successively a P type GaN layer, the 2nd P type GaN layer and the 3rd P type GaN layer on quantum well layer, and it is not identical with the step S2 in embodiment 1 to anneal, step S2 is in the present embodiment:
Be cooled to 750 ℃ by 40s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the P type GaN layer of mixing magnesium that growth thickness is 50 nanometers, wherein the doping content of Mg is 7E+19atom/cm
3;
Be warming up to 920 ℃ by 70s, chamber pressure is controlled at 150mbar, at N
2under atmosphere, the 2nd P type GaN layer of mixing Al and Mg that growth thickness is 40 nanometers, wherein the doping content of Al is 1E+20atom/cm
3, the doping content of Mg is 1E+19atom/cm
3;
Be warming up to 1000 ℃ by 60s, chamber pressure is controlled at 200mbar, at N
2under atmosphere, the 3rd P type GaN layer of mixing Mg that growth thickness is 150 nanometers, wherein the doping content of Mg is 1E+19atom/cm
3;
Annealed, concrete technology is: be cooled to 730 ℃ by 300s, chamber pressure is that 600mbar is at N
2be incubated 20min under atmosphere.
Product test:
Embodiment 1 to 7 and the obtained LED chip of Comparative Examples 1 are carried out to attenuate, then cut into the chip particle of 1143 μ m*1143 μ m (45mi*45mil), and select 150 crystal grain, be packaged into white light LEDs.Under drive current 350mA condition, the brightness, driving voltage and the hole concentration that adopt point measurement machine to test obtained LED.
One, the product test result of embodiment 1 and Comparative Examples 1
Fig. 1 shows the test result signal of the LED product brightness that the embodiment of the present invention 1 and Comparative Examples 1 provide.As shown in Figure 1, the brightness of Comparative Examples 1 resulting LED is 240～250mw, and the brightness of embodiment 1 resulting LED is 256～268mv.Visible, with Comparative Examples 1, resulting LED compares, the luminance raising of embodiment 1 resulting LED 5%～6%.
Fig. 2 shows the test result schematic diagram of the LED product driving voltage that the embodiment of the present invention 1 and Comparative Examples 1 provide.From Fig. 2 data, can draw, the driving voltage of Comparative Examples 1 resulting LED is 3.4～3.5V, and the driving voltage of embodiment 1 resulting LED is 3.25～3.4V.Visible, with Comparative Examples 1, resulting LED compares, and the driving voltage of embodiment 1 resulting LED has reduced by 0.1～0.15V.
Fig. 3 shows the test result schematic diagram of the LED product hole concentration that the embodiment of the present invention 1 and Comparative Examples 1 provide.As shown in Figure 3, when etching depth is less than 0.15 μ m, the hole concentration of Comparative Examples 1 and embodiment 1 is almost equal, and hole concentration has high value (1.5E+17～2.2E+18atom/cm
3), this is because the Mg-H key on close P type GaN surface almost completely interrupts, and makes the hole concentration value higher; In etching depth is 0.15～0.28 μ m scope, the hole concentration of Comparative Examples 1 resulting LED is 1.1E+17～1.2E+17atom/cm
3, and the hole concentration of embodiment 1 resulting LED is 1.3E+17～1.5E+17atom/cm
3, the whole hole concentration of the visible LED obtained by the manufacture method of LED epitaxial wafer provided by the invention effectively improves.
Two, the properties of product of the product of embodiment 1-7 and Comparative Examples 1 contrast
Test result to embodiment 1 to 7 and Comparative Examples 1 obtained LED is averaged, and the mean value that obtains brightness, driving voltage and hole concentration converges, so that the properties of product of the product of embodiment 1-7 and Comparative Examples 1 are analyzed.Concrete outcome is asked for an interview table 1.
Table 1
As can be seen from Table 1, the above embodiments of the present invention have realized following technique effect: with Comparative Examples 1, obtained LED compares, the mean flow rate of the embodiment of the present invention 1～7 obtained LED has improved 13～21mv, average drive voltage has reduced by 0.1～0.14V, and mean void concentration (degree of depth is 0.15～0.28 μ m) has improved 2.3E+16～2.7E+16atom/cm
3.
The above-mentioned execution mode of the present invention has been realized following technique effect: adopt the crystalline quality of whole P type GaN layer in the resulting LED of manufacture method of LED epitaxial wafer provided by the invention to be improved, improved the activation efficiency of whole P type GaN layer Mg, improve hole concentration and the injection efficiency of P layer, make LED chip brightness improve, driving voltage reduces.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. the manufacture method of a LED epitaxial wafer, be included in the step that substrate surface outwards forms U-shaped GaN layer, N-type GaN layer, quantum well layer and a P type GaN layer, the 2nd P type GaN layer and the 3rd P type GaN layer successively, it is characterized in that, described manufacture method also comprises annealing steps, and described annealing steps comprises:
After forming a described P type GaN layer, form the annealing steps at least one times carried out before described the 3rd P type GaN layer; And
Forming another annealing steps carried out after described the 3rd P type GaN layer.
2. manufacture method according to claim 1, is characterized in that, in described annealing steps,
After forming a described P type GaN layer, to form the annealing steps carried out before described the 3rd P type GaN layer be one or many, when this annealing steps is one time, its duration is not less than 120s; When this annealing steps, for repeatedly the time, repeatedly total duration of described annealing steps is no more than 360s, and the duration of the described annealing steps of single is not less than 120s; And
In another annealing steps carried out after forming described the 3rd P type GaN layer, the time of described annealing is 15～25min.
3. manufacture method according to claim 2, is characterized in that, described annealing steps comprises:
Carry out the first annealing steps after forming a described P type GaN layer, preferably, this first annealing steps comprises: in temperature, be 750～760 ℃, and the N that pressure is 200～300mbar
2be incubated 240～300s under atmosphere; And
Carry out the second annealing steps after forming described the 3rd P type GaN layer, preferably, this second annealing steps comprises: be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 20～25min under atmosphere.
4. manufacture method according to claim 2, is characterized in that, described annealing steps comprises:
Carry out the first annealing steps after forming described the 2nd P type GaN layer, preferably, this first annealing steps comprises: be cooled to 760～800 ℃ by 40～60s, the N that is 600～800mbar at pressure
2be incubated 300～360s under atmosphere; And
Carry out the second annealing steps after forming described the 3rd P type GaN layer, preferably, this second annealing steps comprises: being cooled to 730～780 ℃ by 300～320s, is 600～800mbar N at pressure
2be incubated 20～25min under atmosphere.
5. manufacture method according to claim 2, is characterized in that, described annealing steps comprises:
Carry out the first annealing steps after forming a described P type GaN layer, preferably, this first annealing steps comprises: in temperature, be 750～760 ℃, and the N that pressure is 200～300mbar
2be incubated 120～150s under atmosphere;
Carry out the second annealing steps after forming described the 2nd P type GaN layer, preferably, this second annealing steps comprises: be cooled to 760～800 ℃ by 40～60s, the N that is 600～800mbar at pressure
2be incubated 150～180s under atmosphere; And
Carry out the 3rd annealing steps after forming described the 3rd P type GaN layer, preferably, the 3rd annealing steps comprises: be cooled to 730～780 ℃ by 300～320s, the N that is 600～800mbar at pressure
2be incubated 15～20min under atmosphere.
6. according to the described manufacture method of any one in claim 1 to 5, it is characterized in that,
A described P type GaN layer is the P type GaN layer of mixing Mg that thickness is 50～60 nanometers, and wherein the doping content of Mg is 7E+19～1E+20atom/cm
3;
Described the 2nd P type GaN layer is the P type GaN layer of mixing Al and Mg that thickness is 40～50 nanometers, and wherein the doping content of Al is 1E+20～2E+20atom/cm
3, the doping content of Mg is 1E+19～2E+19atom/cm
3;
Described the 3rd P type GaN layer is the P type GaN layer of mixing Mg that thickness is 150～200 nanometers, and wherein the doping content of Mg is 1E+19～5E+19atom/cm
3.
7. manufacture method according to claim 6, is characterized in that,
The step that forms a described P type GaN layer comprises: be cooled to 750～760 ℃ by 40～50s, the N that is 200～300mbar at pressure
2under atmosphere, a described P type GaN layer of magnesium is mixed in growth;
The step that forms described the 2nd P type GaN layer comprises: be warming up to 920～970 ℃ by 70～90s, the N that is 150～300mbar at pressure
2under atmosphere, described the 2nd P type GaN layer of Al and Mg is mixed in growth;
The step that forms described the 3rd P type GaN layer comprises: being warming up to 1000～1100 ℃ by 60～70s, is 200～600mbar at pressure at N
2under atmosphere, described the 3rd P type GaN layer of Mg is mixed in growth.
8. a LED epitaxial wafer, is characterized in that, described LED epitaxial wafer is made by the described manufacture method of any one in claim 1 to 7.
9. a LED chip, comprise epitaxial wafer, P electrode, N electrode and protective layer, it is characterized in that, described epitaxial wafer is the epitaxial wafer described in claim 8.
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